Hydrogen Bromide → HCID 15672517, compound

225 g (1.46 mol) of cyclopropyl-2-thienylcarbinol were added dropwise to 972 ml of 48% strength hydrobromic acid at from 5° to 10° C.in the course of 1 hour. After 2 hours at room temperature, the organic phase was separated off and the aqueous solution was extracted with three times 300 ml of dichloromethane. The combined organic phases were washed neutral with dilute sodium hydroxide solution and water, dried over magnesium sulfate and evaporated down under reduced pressure. 322 g (94% corrected) of crude bromide (GC: 92%) were obtained. 250 MHz-1H-NMR (in CDCl3): δ [ppm]=2.65-2.80 (m, 2H), 3.46 (t, 2H), 5.90-6.10 (m, 1H), 6.61 (d, 1H), 6.80-7.00 (m, 2H), 7.14 (d, 1H).

1. customin the course of 1 hour
2. customthe organic phase was separated off
3. extractionthe aqueous solution was extracted with three times 300 ml of dichloromethane
4. washThe combined organic phases were washed neutral with dilute sodium hydroxide solution and water
5. dry with materialdried over magnesium sulfate
6. customevaporated down under reduced pressure

ORD record

ord-0a48e05b9d484bfbb79220803dc60939

Source dataset

uspto-grants-1996_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05491123